EP1230159A1 - Method for formulating food grade sodium bicarbonate - Google Patents
Method for formulating food grade sodium bicarbonateInfo
- Publication number
- EP1230159A1 EP1230159A1 EP00972494A EP00972494A EP1230159A1 EP 1230159 A1 EP1230159 A1 EP 1230159A1 EP 00972494 A EP00972494 A EP 00972494A EP 00972494 A EP00972494 A EP 00972494A EP 1230159 A1 EP1230159 A1 EP 1230159A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sodium bicarbonate
- set forth
- filtrate
- ammonium
- bicarbonate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/24—Crystallisation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S423/00—Chemistry of inorganic compounds
- Y10S423/09—Reaction techniques
- Y10S423/14—Ion exchange; chelation or liquid/liquid ion extraction
Definitions
- the present invention relates to a method for formulating food grade sodium bicarbonate and more particularly, the present invention relates to a method for formulating food grade sodium bicarbonate by ion exchange purification of sodium bicarbonate.
- soda ash is typically treated with carbon dioxide or purified from product formed in the Solvay process.
- the compound In order to formulate food grade sodium bicarbonate, the compound must be purified to leave a product having less than 100 ppm impurities.
- the prior art has addressed this need in many ways, however, the methods include the use of several unit operations, expensive equipment, high energy input among other factors all contributing to the cost of processing.
- One object of the present invention is to provide an improved method for formulating food grade sodium bicarbonate.
- a further object of one embodiment of the present invention is to provide a method for formulating food grade sodium bicarbonate by purification, comprising the steps of: a) providing a saturated feedstock of sodium bicarbonate, the sodium bicarbonate containing at least sodium sulfate as an impurity; b) filtering the saturated feedstock to remove impurities to form a first filtrate; c) passing the filtrate through an ion exchanger containing a chelating cationic resin to reduce calcium and magnesium ion concentration present in the filtrate; d) cooling the filtrate while introducing a source of ammonia or ammonium ions and carbon dioxide to retain ammonium sulfate in the filtrate and precipitating sodium bicarbonate; and e) filtering precipitated sodium bicarbonate.
- the processes as discussed herein offer a straightforward method of purifying sodium bicarbonate to the food grade standard using ion exchange solubility shifting with reduced levels of energy.
- a method for formulating food grade sodium bicarbonate by purification comprising the steps of: a) providing a saturated feedstock of sodium bicarbonate, the sodium bicarbonate containing at least sodium sulfate, calcium and magnesium as an impurities; b) filtering the saturated feedstock to remove impurities to form a first filtrate; c) passing the filtrate through an ion exchanger containing a chelating cationic resin to reduce calcium and magnesium ion concentration present in the filtrate to less than 10 parts per million; d) cooling the filtrate while introducing a source of ammonia or ammonium ions and carbon dioxide to retain ammonium sulfate in the filtrate and precipitating sodium bicarbonate; and e) filtering precipitated sodium bicarbonate.
- the liquor is progressively purified without risking the introduction of additional impurities to the liquor.
- Figure 1 illustrates a schematic representation of the method according to one embodiment of the present invention.
- FIG. 1 shown is an overall schematic representation of the process according to one embodiment.
- sodium bicarbonate having a purity of 98% which may be contaminated with color impurities, sulfates, sodium sulfate in a range of between 0% by weight and 5% by weight, chlorides, calcium, magnesium, silicon, iron inter alia and is therefore unsuitable as food grade, is dissolved in a vessel 10 containing deionized water at a temperature of between 90°C and 10 ⁇ 'C to the point of saturation. Typically, 15% by weight is added with saturation approximating 20% by weight.
- the liquor is filtered using activated carbon filter 12 containing carbon in a size range of between 80 mesh and 300 mesh. Alternatively, an activated carbon leaf filter may be employed. This step ensures the removal of insolubles, residual organics and any color impurities. The latter are discarded; the filtrate is treated with a series of ion exchange steps for further purification.
- the filtrate from filter 12 is passed into an ion exchange column 14, containing sodium cations.
- the resin is useful to remove calcium and magnesium ion concentrations to less than 10 ppm. The typical values approximate 1 ppm.
- the resin may be regenerated by passing solution 16 on to known arrangements for regeneration purposes.
- the solution exits column 14 at 16 it is passed into a surge tank 20 and subsequently into evaporator 22 where ammonium and water are recovered at 24.
- the solution is then treated in crystallizer 24 to which is added a source of ammonium ions and carbon dioxide.
- a source of ammonium ions and carbon dioxide Use of ammonium bicarbonate may be employed.
- the source of ammonium By making use of the source of ammonium, the result is that the sodium sulfate present as a contaminant is reacted with it to produce ammonium sulfate in solution. This facilitates the precipitation of sodium bicarbonate having significantly reduced sulfate occlusions.
- the temperature of crystallizer 24 may be kept in the range of between 30'C and 70 * C and desirably 40 * C.
- the sodium bicarbonate crystals are grown in a size distribution of -28 mesh and 150 mesh with 60% of the product being in the 60 mesh size distribution.
- the crystals are collected in a cyclone 26 with overflow being recycled via line 28 to tank 20 and subsequently evaporator 22.
- a sulfate ion bleed may be present at 30.
- the crystals from cyclone 26 are passed into a repulp tank 32, a further cyclone 34 and washed at 36. Materials are recycled where indicated and the wash water or repulp vessel may contain approximately 1% ammonium bicarbonate. With adequate retention time, typically 60 minutes at a temperature of between 25 ° C and 50 ° C and most desirably 40 ° C, any residual sulfate ions remain in the ammonium sulfate form. The slurry is then cycloned and centrifuged.
- the product may then be dried in drier 38 with evolved ammonia and water recovered.
- the dryer 38 is maintained a temperature of between 60 ° C and 80 ° C to prevent calcination of sodium bicarbonate to sodium carbonate and releases ammonium bicarbonate to the dryer exit gas.
- the present technology therefore, solves one of the most difficult problems associated with food grade sodium bicarbonate, namely the reduction of sulfate occlusions.
- the methodology herein provides an expeditious procedure without complicated unit operations and high energy input to formulate food grade sodium bicarbonate.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Non-Alcoholic Beverages (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Seasonings (AREA)
- Medicinal Preparation (AREA)
- Fodder In General (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US425968 | 1999-10-25 | ||
US09/425,968 US6475458B1 (en) | 1999-10-25 | 1999-10-25 | Method for formulating food grade sodium bicarbonate |
PCT/CA2000/001266 WO2001030698A1 (en) | 1999-10-25 | 2000-10-24 | Method for formulating food grade sodium bicarbonate |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1230159A1 true EP1230159A1 (en) | 2002-08-14 |
EP1230159B1 EP1230159B1 (en) | 2005-01-19 |
Family
ID=23688760
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00972494A Expired - Lifetime EP1230159B1 (en) | 1999-10-25 | 2000-10-24 | Method for formulating food grade sodium bicarbonate |
Country Status (7)
Country | Link |
---|---|
US (1) | US6475458B1 (en) |
EP (1) | EP1230159B1 (en) |
AT (1) | ATE287378T1 (en) |
AU (1) | AU1121701A (en) |
DE (1) | DE60017581D1 (en) |
MX (1) | MXPA02004086A (en) |
WO (1) | WO2001030698A1 (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20090291038A1 (en) * | 2008-05-23 | 2009-11-26 | Solvay (Societe Anonyme) | Process For The Joint Production of Sodium Carbonate and Sodium Bicarbonate |
MX337503B (en) | 2008-05-13 | 2016-03-03 | Solvay | Process for the joint production of sodium carbonate and sodium bicarbonate. |
CN104707451B (en) * | 2014-12-08 | 2017-04-26 | 华北电力大学(保定) | Method for ammonia-process capture of carbon in flue gas and synthesis of chemical products |
CN106865571B (en) * | 2017-03-20 | 2023-07-25 | 科莱环境工程(北京)有限公司 | Method for preparing sodium bicarbonate and ammonium sulfate from chemical concentrated brine |
CN108862333B (en) * | 2018-09-04 | 2021-03-09 | 北京烨晶科技有限公司 | Process for preparing sodium bicarbonate |
CN113912084B (en) * | 2021-12-09 | 2022-03-04 | 中国科学院过程工程研究所 | Method for preparing sodium carbonate, ammonium sulfate and ammonium chloride by using mixed salt of sodium sulfate and sodium chloride |
Family Cites Families (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3206297A (en) | 1963-03-01 | 1965-09-14 | Standard Oil Co | Slow release fertilizers |
US3493329A (en) | 1966-03-30 | 1970-02-03 | Edouard Louis Stiers | Method of making sodium carbonate |
US3423171A (en) | 1966-06-14 | 1969-01-21 | Kali Forschungs Inst | Method for making alkali metal sulfate |
US3553100A (en) | 1968-09-18 | 1971-01-05 | Shell Oil Co | Upgrading of oil recovered from bituminous sands |
US3728438A (en) | 1970-09-03 | 1973-04-17 | G Nasyrov | Method of producing potassium sulphate from alkali metal sulphates or their mixtures with carbonates |
JPS5641673B2 (en) * | 1972-07-04 | 1981-09-29 | ||
US4385920A (en) | 1976-12-02 | 1983-05-31 | International Minerals & Chemical Corp. | Granulation of potash salts |
US4371512A (en) | 1981-02-03 | 1983-02-01 | Pennzoil Company | Production of alkali metal sulfates |
JPS6259525A (en) * | 1985-09-11 | 1987-03-16 | Tokuyama Soda Co Ltd | Production of sodium bicarbonate |
US4702805A (en) * | 1986-03-27 | 1987-10-27 | C-I-L Inc. | Production of sodium chlorate |
JPH0621033B2 (en) * | 1989-06-12 | 1994-03-23 | セントラル硝子株式会社 | Manufacturing method of high-purity sodium carbonate |
US5654351A (en) | 1990-12-18 | 1997-08-05 | Ormiston Mining And Smelting Co. Ltd. | Method for sodium carbonate compound recovery and formation of ammonium sulfate |
GB9125044D0 (en) * | 1991-11-26 | 1992-01-22 | Brunner Mond & Co Ltd | Production of alkali metal carbonates |
US5830422A (en) | 1995-06-23 | 1998-11-03 | Ormiston Mining And Smelting Co. Ltd. | Method for production of sodium bicarbonate, sodium carbonate and ammonium sulfate from sodium sulfate |
WO1997011907A1 (en) * | 1995-09-29 | 1997-04-03 | Oci Chemical Corp. | Inorganic impurities removal in soda ash solutions with activated carbon |
US5588713A (en) | 1995-12-20 | 1996-12-31 | Stevenson; Tom D. | Process for making sodium bicarbonate from Nahcolite-rich solutions |
CA2284967A1 (en) | 1998-10-13 | 2000-04-13 | Aristos Capital Corporation | Method of formulating alkali earth salts |
-
1999
- 1999-10-25 US US09/425,968 patent/US6475458B1/en not_active Expired - Fee Related
-
2000
- 2000-10-24 DE DE60017581T patent/DE60017581D1/en not_active Expired - Lifetime
- 2000-10-24 AT AT00972494T patent/ATE287378T1/en not_active IP Right Cessation
- 2000-10-24 EP EP00972494A patent/EP1230159B1/en not_active Expired - Lifetime
- 2000-10-24 MX MXPA02004086A patent/MXPA02004086A/en not_active Application Discontinuation
- 2000-10-24 WO PCT/CA2000/001266 patent/WO2001030698A1/en active IP Right Grant
- 2000-10-24 AU AU11217/01A patent/AU1121701A/en not_active Abandoned
Non-Patent Citations (1)
Title |
---|
See references of WO0130698A1 * |
Also Published As
Publication number | Publication date |
---|---|
AU1121701A (en) | 2001-05-08 |
WO2001030698A1 (en) | 2001-05-03 |
MXPA02004086A (en) | 2004-03-26 |
US6475458B1 (en) | 2002-11-05 |
ATE287378T1 (en) | 2005-02-15 |
DE60017581D1 (en) | 2005-02-24 |
EP1230159B1 (en) | 2005-01-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105293588B (en) | Preparation method for battery grade ferrous sulfate heptahydrate crystal | |
US4222989A (en) | Method for the manufacture of pure aluminum oxide from aluminum ore | |
RU2176218C2 (en) | Method of production of potassium sulfate and sodium sulfate (versions) | |
US3899571A (en) | Method for the removal of organic substances from sodium aluminate solution | |
CN110563003B (en) | Method and apparatus for treating waste liquid from polarizing plate production | |
EP1230159B1 (en) | Method for formulating food grade sodium bicarbonate | |
US4597952A (en) | Purification of solutions of sodium aluminate in the Bayer cycle by the removal of sodium oxalate | |
US3852044A (en) | Recovery of substantially potassium-free hydrated magnesium chloride from contaminated aqueous solutions | |
KR20150076087A (en) | Production processes of high-purity sodium hypochlorite pentahydrate and aqueous sodium hypochlorite solution | |
US6106796A (en) | Method of ammonium sulfate purification | |
CN112142068A (en) | Method for producing high-purity ammonium chloride from industrial-grade ammonium chloride | |
MXPA96004583A (en) | Process for the recovery of the salon bathroom components of the detem workshops | |
JP4275939B2 (en) | Method for recovering tantalum compound and / or niobium compound | |
CA2181613C (en) | Impurity removal from sodium chlorate | |
EP0127262B1 (en) | Purification of bayer process liquors | |
US2863809A (en) | Process for concentration of caustic cell liquor | |
US3642455A (en) | Process for recovering low-sulfate bischofite | |
CN113443762A (en) | Method for treating waste liquid from manufacture of polarizing plate | |
US3337305A (en) | Purifying caustic aluminate solutions with ammonia | |
JP3257105B2 (en) | Method for producing zirconium oxychloride crystal | |
US3498758A (en) | Method of recovering strontium chloride | |
JP4322008B2 (en) | Method for recovering tantalum compound and / or niobium compound | |
JP3137226B2 (en) | Production method of high purity strontium chloride | |
JP2960876B2 (en) | Copper electrolyte cleaning method | |
SU1303631A1 (en) | Method for extracting copper from used copper-ammoniate pickling solutions |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20020516 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE |
|
AX | Request for extension of the european patent |
Free format text: AL PAYMENT 20020516;LT PAYMENT 20020516;LV PAYMENT 20020516;MK PAYMENT 20020516;RO PAYMENT 20020516;SI PAYMENT 20020516 |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE |
|
AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 Ref country code: LI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 Ref country code: IT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED. Effective date: 20050119 Ref country code: FR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20050119 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 Ref country code: CH Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 Ref country code: BE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050119 |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D |
|
REF | Corresponds to: |
Ref document number: 60017581 Country of ref document: DE Date of ref document: 20050224 Kind code of ref document: P |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050419 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050419 Ref country code: DK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050419 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050420 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20050430 |
|
LTIE | Lt: invalidation of european patent or patent extension |
Effective date: 20050119 |
|
NLV1 | Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act | ||
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051024 Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051024 Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20051024 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051031 Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051031 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed |
Effective date: 20051020 |
|
EN | Fr: translation not filed | ||
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20051024 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: MM4A |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20050619 |